Potassium Carbonate → 7-Benzyloxy-4-(2,3-dimethylindol-5-yloxy)-6-methoxyquinazoline

HRID 1791624

反応式

HRID 1791624 の反応式
[CH3:1][C:2]1[NH:3][C:4]2[C:9]([C:10]=1[CH3:11])=[CH:8][C:7]([OH:12])=[CH:6][CH:5]=2.C(=O)([O-])[O-].[K+].[K+].[CH2:19]([O:26][C:27]1[CH:36]=[C:35]2[C:30]([C:31](Cl)=[N:32][CH:33]=[N:34]2)=[CH:29][C:28]=1[O:38][CH3:39])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>CN(C=O)C>[CH2:19]([O:26][C:27]1[CH:36]=[C:35]2[C:30]([C:31]([O:12][C:7]3[CH:8]=[C:9]4[C:4](=[CH:5][CH:6]=3)[NH:3][C:2]([CH3:1])=[C:10]4[CH3:11])=[N:32][CH:33]=[N:34]2)=[CH:29][C:28]=1[O:38][CH3:39])[C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 106619987-(Benzyloxy)-4-chloro-6-methoxyquinazolineHCID 220307882,3-Dimethyl-1H-indol-5-ol

生成物 1

HCID 220308297-Benzyloxy-4-(2,3-dimethylindol-5-yloxy)-6-methoxyquinazoline収率 98.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Under nitrogen, to a solution of 2,3-dimethyl-5-hydroxyindole (643 mg, 4 mmol), in DMF (10 ml) was added potassium carbonate (690 mg, 5 mmol). After stirring for 15 minutes at ambient temperature, 7-benzyloxy-4-chloro-6-methoxyquinazoline (1 g, 3.33 mmol), (prepared as described for the starting material in Example 1), was added. The mixture was heated at 90° C. for 2 hours followed by 30 minutes at 95° C. After cooling, the mixture was poured onto water (100 ml) cooled at 5° C. The precipitate was filtered, washed with water, followed by ether and dried under vacuum to give 7-benzyloxy-4-(2,3-dimethylindol-5-yloxy)-6-methoxyquinazoline (1.4 g, 95%).

後処理

  1. additionwas added
  2. temperatureThe mixture was heated at 90° C. for 2 hours
  3. waitfollowed by 30 minutes at 95° C
  4. temperatureAfter cooling
  5. additionthe mixture was poured onto water (100 ml)
  6. temperaturecooled at 5° C
  7. filtrationThe precipitate was filtered
  8. washwashed with water
  9. customdried under vacuum

出典と根拠

ORDレコード
ord-42046bf8cb5d4a69a8401106f59e4bd4
出典データセット
uspto-grants-2006_07
特許番号
US07074800B1

関連ノート

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